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电感耦合等离子体质谱法测定煤和大气颗粒物中的碘和溴。

Determination of iodine and bromine in coal and atmospheric particles by inductively coupled plasma mass spectrometry.

机构信息

Technique Test Lab., Shanghai Entry-Exit Inspection and Quarantine Bureau, No. 1208, Minsheng Road, Pudong New District, Shanghai 200135, China.

出版信息

Talanta. 2010 Apr 15;81(1-2):473-6. doi: 10.1016/j.talanta.2009.12.026. Epub 2009 Dec 23.

Abstract

Bromine and iodine in atmospheric particles or coal can cause environmental problems such as destruction of ozone in the atmosphere; therefore, the presence of these compounds has recently received increased attention. Here, a rapid and reliable method for the simultaneous determination of total bromine and iodine using ICP-MS analysis is described. Samples were dissolved in mixtures of 5 mL of HNO(3) and 2 mL of H(2)O(2) in a high pressure microwave digester. The solution was then oxidized by per-sulfate (Na(2)S(2)O(8)) in addition to a small amount of silver nitrate, after which the total bromine and iodine were measured simultaneously by ICP-MS. The signal memory effects of bromine and iodine during analysis were effectively decreased by washing with a new mixture agent (2% alcohol acidic solution, pH 1-2 adjusted with HCl). The detection limits for bromine and iodine using this method were about 3.2 microg L(-1) and 1.1 microg L(-1), respectively. Additionally, the spike recoveries were between 78.7% and 121% for bromine and iodine analysis, while the relative standard deviations ranged from 4.3% to 9.7%, and from 1.5% to 3.4% for bromine and iodine, respectively. The results of this study indicate that the method described here is suitable for the analysis of micro-amounts of bromine and iodine in atmospheric particles and coal samples.

摘要

大气颗粒物或煤中的溴和碘会引起环境问题,如大气中臭氧的破坏;因此,这些化合物最近受到了越来越多的关注。本文描述了一种利用 ICP-MS 分析同时测定总溴和碘的快速可靠方法。样品在高压微波消解罐中用 5 mL HNO3 和 2 mL H2O2 的混合物溶解。然后在少量硝酸银存在下,用过硫酸盐(Na2S2O8)将溶液氧化,之后通过 ICP-MS 同时测定总溴和碘。通过用新的混合剂(2%酸性酒精溶液,用 HCl 调节 pH 值为 1-2)冲洗,可以有效降低分析过程中溴和碘的信号记忆效应。该方法测定溴和碘的检出限分别约为 3.2 μg/L 和 1.1 μg/L。此外,溴和碘的加标回收率分别在 78.7%至 121%之间,相对标准偏差分别在 4.3%至 9.7%和 1.5%至 3.4%之间。研究结果表明,本文所述方法适用于大气颗粒物和煤样品中痕量溴和碘的分析。

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